CN117466626B - Method for preparing magnesium-based composite refractory bricks by recycling waste magnesia carbon bricks - Google Patents
Method for preparing magnesium-based composite refractory bricks by recycling waste magnesia carbon bricks Download PDFInfo
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- CN117466626B CN117466626B CN202311811520.6A CN202311811520A CN117466626B CN 117466626 B CN117466626 B CN 117466626B CN 202311811520 A CN202311811520 A CN 202311811520A CN 117466626 B CN117466626 B CN 117466626B
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- 239000011449 brick Substances 0.000 title claims abstract description 220
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 172
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000002699 waste material Substances 0.000 title claims abstract description 94
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 86
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 86
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 37
- 239000011777 magnesium Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004064 recycling Methods 0.000 title claims description 14
- 239000000843 powder Substances 0.000 claims abstract description 118
- 239000000463 material Substances 0.000 claims abstract description 79
- 239000002245 particle Substances 0.000 claims abstract description 64
- 238000003825 pressing Methods 0.000 claims abstract description 62
- 238000002156 mixing Methods 0.000 claims abstract description 43
- 229910021383 artificial graphite Inorganic materials 0.000 claims abstract description 31
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 23
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 23
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 23
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 21
- 239000004917 carbon fiber Substances 0.000 claims abstract description 21
- 239000011294 coal tar pitch Substances 0.000 claims abstract description 21
- 238000004381 surface treatment Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 58
- 239000003963 antioxidant agent Substances 0.000 claims description 35
- 230000003078 antioxidant effect Effects 0.000 claims description 35
- 239000003245 coal Substances 0.000 claims description 28
- 239000001095 magnesium carbonate Substances 0.000 claims description 28
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 28
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 28
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 28
- 239000011295 pitch Substances 0.000 claims description 28
- 238000009987 spinning Methods 0.000 claims description 28
- 229910002804 graphite Inorganic materials 0.000 claims description 22
- 239000010439 graphite Substances 0.000 claims description 22
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 21
- 239000005011 phenolic resin Substances 0.000 claims description 21
- 229920001568 phenolic resin Polymers 0.000 claims description 21
- 229920001187 thermosetting polymer Polymers 0.000 claims description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 238000010304 firing Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000002006 petroleum coke Substances 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- 239000010431 corundum Substances 0.000 claims description 9
- 230000003111 delayed effect Effects 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 9
- 210000002615 epidermis Anatomy 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 5
- 229910001570 bauxite Inorganic materials 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 3
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims description 3
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052599 brucite Inorganic materials 0.000 claims description 3
- 229910021343 molybdenum disilicide Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000000498 ball milling Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 239000011819 refractory material Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 104
- RWDBMHZWXLUGIB-UHFFFAOYSA-N [C].[Mg] Chemical compound [C].[Mg] RWDBMHZWXLUGIB-UHFFFAOYSA-N 0.000 description 8
- 239000011300 coal pitch Substances 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009991 scouring Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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Abstract
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks belongs to the technical field of refractory materials, and comprises the steps of ball milling and modifying waste magnesia carbon brick powder by adopting polyvinylpyrrolidone aqueous solution, mixing and pressing pre-buried blocks with carbon fibers, artificial graphite and coal tar pitch, carrying out surface treatment on the pre-buried blocks, and then layering and pre-burying the pre-buried blocks in refractory brick base materials. According to the invention, the waste magnesia carbon brick material is prepared into the embedded blocks after being subjected to particle modification, and is embedded in the refractory brick, so that various performance indexes can be improved, the oxidation resistance and corrosion resistance of the surface of the refractory brick cannot be affected by the waste magnesia carbon brick material, and after the special treatment is performed for embedding the briquettes, the strength, thermal shock resistance and creep resistance of the refractory brick can be greatly improved, cracks are not easy to occur, and the use level of the high-quality refractory brick can be reached.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a method for preparing magnesium-based composite refractory bricks by recycling waste magnesia carbon bricks.
Background
In the production and manufacture, a kiln is generally used for sintering or smelting products, or a high-temperature resistant container is used for containing high-temperature semi-finished products, so that a large amount of refractory bricks are required to be supplied. With the updating of kiln, maintenance and abandonment, a large number of obsolete refractory bricks, generally waste magnesia carbon bricks, are generated, and some are added and applied to capital construction and building materials, and some are directly treated as garbage. Because the waste magnesia carbon bricks undergo long-term high-temperature oxidation, thermal shock and erosion and corrosion in a kiln or a container, the performances are greatly deteriorated, the waste magnesia carbon bricks are difficult to recycle and recycle in refractory bricks, even if the waste magnesia carbon bricks are recycled, the quality of the refractory bricks can be reduced when the waste magnesia carbon bricks are partially added into new refractory bricks, cracks are extremely easy to occur, the thermal shock resistance, the anti-scouring property, the oxidation resistance, the erosion resistance and the like are low, the regenerated bricks can only be used as low-grade products, and the use quality of the high-quality refractory bricks can not be achieved, so the recycling rate of the waste magnesia carbon bricks is not high.
Under the development direction of cost reduction, quality improvement and synergy and the environment that refractory material resources are gradually exhausted, the utilization rate of the waste magnesia carbon bricks is greatly required to be improved, and the use quality of the recycled bricks is also improved, so that the performance of each index of the recycled bricks doped with the waste magnesia carbon brick materials is comparable to that of high-quality refractory bricks. At present, for recycling treatment of waste magnesia carbon bricks, the use quality of the waste magnesia carbon bricks is improved, and main concerns remain on pretreatment, such as hydration, iron removal, roasting and the like after crushing, so that the quality improvement effect on the recycled bricks is still not ideal.
Disclosure of Invention
The method aims at solving the problems that the prior waste magnesia carbon brick has low resource utilization rate, and the regenerated brick prepared by doping the waste magnesia carbon brick powder has low performance indexes such as thermal shock resistance, anti-scouring, oxidation resistance, erosion resistance and the like. The invention provides a method for preparing magnesium-based composite refractory bricks by recycling waste magnesia carbon bricks, which is characterized in that waste magnesia carbon brick materials are prepared into embedded blocks after being subjected to particle modification, various performance indexes can be improved by embedding the embedded blocks in the refractory bricks, the waste magnesia carbon brick materials can not influence the oxidation resistance and corrosion resistance of the surfaces of the refractory bricks, the strength, the thermal shock resistance and the creep resistance can be greatly improved after being embedded by special treatment of the briquettes, cracks are not easy to occur, and the use level of high-quality refractory bricks can be achieved. The specific technical scheme is as follows:
a method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; according to the mass ratio of the waste magnesia carbon brick powder to the polyvinylpyrrolidone water solution=1 (1.5-3), carrying out corundum ball wet ball grinding on the waste magnesia carbon brick powder for 30-50 min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
according to the mass ratio of (1) modified powder A to (10) to (3-10) to (5-10) of (100) artificial graphite to (5-10) coal tar pitch, mixing the modified powder A with the carbon fiber, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing the mixture into blocks by adopting a die, and sintering and curing the blocks at 1200-1400 ℃ to obtain embedded blocks;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
according to the mass ratio of magnesite powder to zirconia powder to crystalline flake graphite to antioxidant to coal-based spinning pitch=100 (5-10), 5-10, 0-6 and 3-10, mixing the magnesite powder, the zirconia powder, the crystalline flake graphite and the antioxidant, and then adding the coal-based spinning pitch to uniformly mix to obtain a base material B;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing the die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing the die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is more than 20mm from the side edge of the die, then adding the base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing the die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing the die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1200-1500 ℃ and preserving heat for 2-5 hours to obtain the magnesium-based composite refractory bricks.
In the technical scheme S1, the mass concentration of the polyvinylpyrrolidone aqueous solution is 3-15%.
In the above technical scheme S2, the dimensional parameter of the carbon fiber is 2 mm-6 mm in length and 8 um-20 um in diameter.
In the S2 of the technical scheme, the artificial graphite is prepared by sintering delayed petroleum coke powder at 2800-3000 ℃ for 2-5 hours, and the median particle size is below 20um.
In the above technical scheme S2, the median particle size of the coal tar pitch is 3um or less.
In the S2 of the above technical solution, the shape of the embedded block is a cube, a cuboid or a hemisphere, and the side length or the diameter of the embedded block is 10 mm-30 mm.
In the above technical scheme S4, the antioxidant is one or more of boron carbide, silicon carbide, bauxite powder, metallic silicon, brucite powder and molybdenum disilicide.
In the S4 of the technical scheme, the magnesite powder grain size distribution is that 35-45 wt% of particles with the grain diameter of less than 5mm and more than or equal to 3mm, 15-25 wt% of particles with the grain diameter of less than 3mm and more than or equal to 1mm, 10-25 wt% of particles with the grain diameter of less than 1mm and more than or equal to 0.5mm and 5-15 wt% of particles with the grain diameter of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the antioxidant is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um.
In the S5 of the technical scheme, the die head weight pressure is 130 MPa-160 MPa; the pressure of the light pressure of the die head is 15MPa to 25MPa.
Compared with the prior art, the method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks has the beneficial effects that:
1. according to the invention, the recovered waste magnesia carbon bricks are peeled, the surface layer with the thickness of more than 2mm is peeled off and removed, the surface oxidation erosion layer can be removed, the quality of the waste magnesia carbon brick materials is improved, and hydration treatment is not required.
2. According to the invention, wet ball milling is carried out on the waste magnesia carbon brick powder and the polyvinylpyrrolidone aqueous solution, so that on one hand, the particle morphology of the waste magnesia carbon brick powder can be improved, and the strength of the material filling pressing block can be improved; on the other hand, after drying, a layer of polyvinylpyrrolidone can be attached to the surfaces of the waste magnesia carbon brick powder particles, so that the defects of the particle surfaces can be improved, the porosity of the briquettes can be reduced, the bonding strength of the briquettes can be increased, and the thermal shock resistance can be improved.
3. According to the invention, the waste magnesia carbon brick powder subjected to ball milling modification by polyvinylpyrrolidone is mixed and pressed with carbon fiber, artificial graphite and coal pitch, so that the breaking strength, compressive strength and thermal shock resistance and creep resistance of the embedded block can be improved by the carbon fiber and the artificial graphite; the artificial graphite is prepared by adopting the delayed petroleum coke powder to sinter for 2-5 hours at 2800-3000 ℃, has good heat resistance and low creep rate, has better bonding degree with the polyvinylpyrrolidone surface of the waste magnesia carbon brick powder, and can greatly improve bonding compactness and firmness.
4. According to the invention, the surface of the embedded block is uniformly coated with a layer of thermosetting liquid phenolic resin, the pressing combination compactness of the embedded block and the base material can be well ensured by utilizing the viscosity and thermosetting property of the liquid phenolic resin, and the displacement of the embedded block is less or completely eradicated in the pressing process; good homogeneity of the refractory brick is achieved.
5. The invention designs that the embedded block is not exposed on the surface of the refractory brick, and is more than 20mm away from the surface of the refractory brick, the embedded block can be well protected from scouring, erosion and oxidization of the external environment, the long service life of the embedded block is ensured, in addition, the surface of the refractory brick is not influenced by waste magnesia carbon brick powder, the performance is reduced, and the embedded block is easy to oxidize and crack.
6. According to the invention, zirconia powder, crystalline flake graphite and an antioxidant are added into the refractory brick base material to improve the surface performance, and embedded blocks are used, so that indexes such as various strength, thermal shock resistance, oxidation resistance, creep resistance and the like are ensured to reach the use standard of high-quality refractory bricks.
7. The invention also designs a special brick pressing forming process aiming at the embedded block, and soft layers are designed at the lower layers of the embedded block, so that the embedded block can be pressed into the soft layers, and the embedded block is more tightly combined and cannot be layered to crack or break.
8. The invention designs the shape of the embedded block which is a cube, a cuboid or a hemisphere, and the side length or the diameter of the embedded block is 10 mm-30 mm, so that the homogeneity of waste magnesia carbon brick powder and base materials in the refractory brick can be well ensured, and the strength index of the refractory brick can be ensured.
In conclusion, the waste magnesia carbon brick material pressing block is embedded in the refractory brick, so that various performance indexes can be improved, the waste magnesia carbon brick material does not influence the oxidation resistance and corrosion resistance of the surface of the refractory brick, the strength, the thermal shock resistance and the creep resistance can be greatly improved after the special treatment pressing block is embedded, cracks are not easy to occur, the use level of the high-quality refractory brick can be achieved, and the high-quality refractory brick has good practical value.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the invention is not limited to these examples.
Example 1
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with 8% polyvinylpyrrolidone water solution according to the mass ratio of polyvinylpyrrolidone water solution=1:2, performing corundum ball wet ball grinding for 40min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:6:5:6, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and sintering and curing at 1300 ℃ to obtain pre-buried blocks; the shape of the embedded block is cube, and the side length is 20mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 3000 ℃ for 3 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:8:8:3:6, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is boron carbide, and the median particle diameter is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing by a 150MPa die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 20MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is 25mm from the side edge of the die, then adding a base material B again, wherein the addition amount of the base material B is 10mm after the embedded blocks are submerged, and repeatedly pressing a 150MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 150MPa die head to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1300 ℃, and preserving heat for 3 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, 3 layers of embedded blocks are embedded in the brick, and 30 embedded blocks are uniformly distributed on each layer; the volume of the embedded block accounts for more than 10 percent of the volume of the whole refractory brick.
Example 2
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with polyvinylpyrrolidone water solution with the mass concentration of 3% according to the mass ratio of polyvinylpyrrolidone water solution=1:1.5, performing corundum ball wet ball grinding for 30min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:3:3:5, then adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and then sintering and curing at 1200 ℃ to obtain pre-buried blocks; the shape of the embedded block is a hemispherical body, and the diameter is 10mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 2800 ℃ for 2 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:5:5:0:3, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein, the grain size distribution of the magnesite is that the grain with the grain size of less than 5mm and more than or equal to 3mm accounts for 35wt percent to 45wt percent, the grain with the grain size of less than 3mm and more than or equal to 1mm accounts for 15wt percent to 25wt percent, the grain with the grain size of less than 1mm and more than or equal to 0.5mm accounts for 10wt percent to 25wt percent, and the grain with the grain size of less than 0.5mm accounts for 5wt percent to 15wt percent; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing by a 130MPa die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 15MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, enabling the hemispherical plane to be downward, enabling the distance between two adjacent embedded blocks to be more than 5mm, enabling the distance between two adjacent embedded blocks to be 20mm from the side edge of a die, adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing a 130MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 130MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1200 ℃, and preserving heat for 2 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Example 3
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with a polyvinylpyrrolidone aqueous solution with a mass concentration of 15% according to the mass ratio of the waste magnesium carbon brick powder to the polyvinylpyrrolidone aqueous solution=1:3, performing wet ball grinding on corundum balls for 50min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:10:8:10, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and sintering and curing at 1400 ℃ to obtain pre-buried blocks; the shape of the embedded block is a hemispherical body, and the side length is 30mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 3000 ℃ for 5 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to antioxidant to coal-based spinning pitch=100:10:10:6:10, and then adding coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is molybdenum disilicide, and the median particle diameter of the antioxidant is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing by a 160MPa die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 25MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, enabling the hemispherical plane to be downward, enabling the distance between two adjacent embedded blocks to be more than 5mm, enabling the embedded blocks to be 25mm away from the side edge of a die, then adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing a 160MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 160MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1500 ℃ and preserving heat for 5 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Example 4
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with 15% polyvinylpyrrolidone water solution according to the mass ratio of polyvinylpyrrolidone water solution=1:1.5, performing corundum ball wet ball grinding for 30min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:10:3:10, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and sintering and curing at 1200 ℃ to obtain pre-buried blocks; the embedded block is in a cuboid shape, and the length, width and height are 30mm multiplied by 15mm multiplied by 10mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 2800 ℃ for 5 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:5:10:1:10, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is silicon carbide, and the median particle size of the antioxidant is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing by a 130MPa die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 25MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is 22mm from the side edge of the die, then adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing a 130MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 130MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1500 ℃, and preserving heat for 2 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Example 5
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with polyvinylpyrrolidone water solution with the mass concentration of 3% according to the mass ratio of polyvinylpyrrolidone water solution=1:3, performing corundum ball wet ball grinding for 50min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:3:8:5, then adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and then sintering and curing at 1400 ℃ to obtain pre-buried blocks; the shape of the embedded block is 30mm square;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 3000 ℃ for 2 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:10:5:6:3, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is bauxite powder, and the median particle size of the antioxidant is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing by a 160MPa die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 15MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is 30mm from the side edge of the die, then adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing by a 160MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 160MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1200 ℃, and preserving heat for 5 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Example 6
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with a polyvinylpyrrolidone aqueous solution with the mass concentration of 6% according to the mass ratio of polyvinylpyrrolidone aqueous solution=1:1.8, performing corundum ball wet ball grinding for 35min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:4:4:6, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and sintering and curing at 1250 ℃ to obtain pre-buried blocks; the shape of the embedded block is cube, and the side length is 12mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by sintering delayed petroleum coke powder at 2850 ℃ for 2.5 hours, and the median particle diameter is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:6:6:2:4, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is brucite powder, and the median particle size of the antioxidant is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing the die head under 140MPa to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing an 18MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is 24mm from the side edge of the die, then adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing a 140MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 140MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1250 ℃, and preserving heat for 2.5 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Example 7
A method for preparing magnesium-based composite refractory bricks by reutilizing waste magnesia carbon bricks comprises the following steps:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; mixing waste magnesium carbon brick powder with 12% polyvinylpyrrolidone water solution according to the mass ratio of polyvinylpyrrolidone water solution=1:2.5, performing corundum ball wet ball grinding for 45min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
mixing the modified powder A with the carbon fiber according to the mass ratio of the modified powder A to the artificial graphite to the coal tar pitch=100:8:6:8, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing into blocks by adopting a die, and sintering and curing at 1350 ℃ to obtain pre-buried blocks; the shape of the embedded block is a hemispherical body, and the diameter is 25mm;
the size parameters of the carbon fiber are that the length is 2 mm-6 mm and the diameter is 8 um-20 um; the artificial graphite is prepared by retarding petroleum coke powder to sinter at 2900 ℃ for 3 hours, and the median particle size is below 20um; the median granularity of the coal pitch is below 3 um;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
mixing magnesite powder, zirconia powder, crystalline flake graphite and an antioxidant according to the mass ratio of magnesite powder to zirconia powder to an antioxidant to coal-based spinning pitch=100:8:8:5:8, and then adding the coal-based spinning pitch for uniform mixing to obtain a base material B;
wherein the antioxidant is a composition of bauxite powder and metallic silicon in equal mass ratio, and the median particle size of the antioxidant is below 20um; the grain size distribution of the magnesite is that 35-45 wt% of grains with the grain size of less than 5mm and more than or equal to 3mm, 15-25 wt% of grains with the grain size of less than 3mm and more than or equal to 1mm, 10-25 wt% of grains with the grain size of less than 1mm and more than or equal to 0.5mm, and 5-15 wt% of grains with the grain size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 um; the median particle diameter of the flake graphite is below 20um; the median particle diameter of the coal-based spinning pitch is below 3 um;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing the die head at 155MPa to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing a 22MPa die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, enabling the hemispherical plane to be downward, enabling the distance between two adjacent embedded blocks to be more than 5mm, enabling the embedded blocks to be 30mm away from the side edge of a die, then adding a base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing a 155MPa die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing by a 155MPa die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
s6, firing:
and firing the green bricks at 1400 ℃, and preserving heat for 4 hours to obtain the magnesium-based composite refractory bricks.
The specification of the magnesium-based composite refractory brick sample piece of the embodiment is 300mm multiplied by 150mm, and the volume of the embedded block accounts for more than 10% of the volume of the whole refractory brick.
Comparative example 1 was prepared: the waste magnesia carbon brick powder is not subjected to wet ball milling; other parameters were the same as those of the method of example 1.
Comparative example 2 was prepared: the surface of the embedded block is not coated with thermosetting liquid phenolic resin; other parameters were the same as those of the method of example 1.
Comparative example 3 was prepared: the waste magnesia carbon brick powder is not subjected to wet ball milling and is not subjected to pressing of embedded blocks, and the waste magnesia carbon brick powder is directly mixed into the base material B, wherein the mixing ratio is that magnesite powder, waste magnesia carbon brick powder, zirconia powder, crystalline flake graphite, antioxidant and coal-based spinning pitch=87:13:8:8:3:6; other parameters were the same as those of the method of example 1.
The refractory bricks of examples 1 to 7 and comparative examples 1 to 3 were subjected to performance tests, and the results are shown in the following table:
from the above results, it is known that the waste magnesia carbon brick material is embedded in the refractory brick, so that various performance indexes can be improved, the waste magnesia carbon brick material does not affect the oxidation resistance and corrosion resistance of the surface of the refractory brick, and the strength, thermal shock resistance and creep resistance can be greatly improved after the special treatment of the embedded compact.
Claims (7)
1. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks is characterized by comprising the following steps of:
s1, pretreatment of waste magnesia carbon bricks:
peeling the recovered waste magnesia carbon bricks, removing the epidermis layer with the thickness of more than 2mm, crushing the waste magnesia carbon bricks into powder with the thickness of less than 200 mu m, and then demagnetizing; according to the mass ratio of the waste magnesia carbon brick powder to the polyvinylpyrrolidone water solution=1 (1.5-3), carrying out corundum ball wet ball grinding on the waste magnesia carbon brick powder for 30-50 min, filtering and drying to obtain modified powder A;
s2, preparing embedded blocks:
according to the mass ratio of (1) modified powder A to (10) to (3-10) to (5-10) of (100) artificial graphite to (5-10) coal tar pitch, mixing the modified powder A with the carbon fiber, adding the artificial graphite and the coal tar pitch for uniform mixing, pressing the mixture into blocks by adopting a die, and sintering and curing the blocks at 1200-1400 ℃ to obtain embedded blocks;
the artificial graphite is prepared by sintering delayed petroleum coke powder at 2800-3000 ℃ for 2-5 hours, and the median particle size is below 20 mu m;
s3, surface treatment of the embedded block:
uniformly coating a layer of thermosetting liquid phenolic resin on the surface of the embedded block, wherein the coating amount is that the thermosetting liquid phenolic resin does not flow when each surface of the embedded block is vertically placed;
s4, preparing a base material:
according to the mass ratio of magnesite powder to zirconia powder to crystalline flake graphite to antioxidant to coal-based spinning pitch=100 (5-10), 5-10, 0-6 and 3-10, mixing the magnesite powder, the zirconia powder, the crystalline flake graphite and the antioxidant, and then adding the coal-based spinning pitch to uniformly mix to obtain a base material B;
s5, pressing refractory bricks:
s5.1: adding a layer of base material B into a brick die cavity, and pressing the die head to form a hard layer;
s5.2: adding a layer of base material B again, and lightly pressing the die head to form a soft layer;
s5.3: uniformly laying a plurality of embedded blocks, wherein the distance between two adjacent embedded blocks is more than 5mm, the distance between the embedded blocks is more than 20mm from the side edge of the die, then adding the base material B again, wherein the addition amount of the base material B is more than 5mm after the embedded blocks are submerged, and repeatedly pressing the die head to form a hard layer; at this time, the embedded block is partially embedded in the soft layer, and the soft layer is pressed into a hard layer;
s5.4: adding a layer of base material B again, and pressing the die head again to form a hard layer;
s5.5: repeating the steps S5.2 to S5.4 for more than two times until the refractory bricks are pressed, and obtaining green bricks;
the die head weight pressure is 130-160 MPa; the pressure of the light pressure of the die head is 15MPa to 25MPa;
s6, firing:
and firing the green bricks at 1200-1500 ℃ and preserving heat for 2-5 hours to obtain the magnesium-based composite refractory bricks.
2. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in S1, the mass concentration of the polyvinylpyrrolidone aqueous solution is 3-15%.
3. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in S2, the dimension parameter of the carbon fiber is 2 mm-6 mm in length and 8-20 μm in diameter.
4. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in S2, the median particle size of the coal tar pitch is below 3 μm.
5. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in the S2, the shape of the embedded block is a cube, a cuboid or a hemisphere, and the side length or the diameter of the embedded block is 10-30 mm.
6. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in the step S4, the antioxidant is one or a combination of more of boron carbide, silicon carbide, bauxite powder, metallic silicon, brucite powder and molybdenum disilicide.
7. The method for preparing the magnesium-based composite refractory brick by recycling the waste magnesia carbon bricks according to claim 1, wherein in S4, the particle size distribution of the magnesite powder is that 35-45 wt% of particles with the particle size of less than 5mm and more than or equal to 3mm, 15-25 wt% of particles with the particle size of less than 3mm and more than or equal to 1mm, 10-25 wt% of particles with the particle size of less than 1mm and more than or equal to 0.5mm and 5-15 wt% of particles with the particle size of less than 0.5 mm; the median particle diameter of the zirconia powder is below 30 mu m; the median particle diameter of the flake graphite is below 20 mu m; the median particle diameter of the antioxidant is below 20 μm; the median particle diameter of the coal-based spinning pitch is 3 μm or less.
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CN104446530A (en) * | 2014-10-27 | 2015-03-25 | 朱小英 | Preparation process for refractory brick on ladle slag line |
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